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[目的]建立黄瓜花粉中氟啶虫胺腈的残留分析方法,为氟啶虫胺腈的安全使用提供技术支撑。[方法]前处理方法利用乙腈为提取剂,正己烷作为脱脂剂,N-丙基乙二胺(PSA)和石墨化炭黑(GCB)为分散净化剂的QuEChERS方法,并利用超高效液相色谱-串联质谱(UPLC-MS/MS)在多反应离子监测模式(MRM)下进行检测,外标法定量。[结果]氟啶虫胺腈在0.001~0.500 mg/L质量浓度范围内均具有良好的线性关系;在0.01~1.00 mg/kg添加水平范围内平均回收率为80.33%~99.55%;相对标准偏差为4.7%~7.5%;方法检出限(LOD)为0.0018 mg/kg;定量限(LOQ)在0.006 mg/kg。[结论]该方法分析速度快、灵敏度高、重现性好,适用于黄瓜花粉中氟啶虫胺腈的快速检测和确证。
[Objective] The research aimed to establish a method for the residual analysis of flonidase in cucumber pollen and provide technical support for its safe use. [Method] The pretreatment method used QuEChERS method with acetonitrile as extractant, n-hexane as degreasing agent, N-propyl ethylenediamine (PSA) and graphitized carbon black (GCB) as dispersing and purifying agent, Chromatography-tandem mass spectrometry (UPLC-MS / MS) was performed in multiple reaction ion monitoring (MRM) mode and quantified by external standard method. [Result] The results showed that there was a good linear relationship between the concentration of nitrofen and nitrite in the range of 0.001-0.500 mg / L. The average recoveries were between 80.33% and 99.55% in the range of 0.01-1.00 mg / kg. The relative standard deviation Was 4.7% ~ 7.5%. The limit of detection (LOD) was 0.0018 mg / kg. The limit of quantification (LOQ) was 0.006 mg / kg. [Conclusion] The method was rapid, sensitive and reproducible. It was suitable for the rapid detection and confirmation of flurbaron in cucumber pollen.